Lubricating composition



Feb, M 11928.

E. A. NlLL LUBRICATING COMPOSITION Filed May 4, 1923 Patented Feb. 14,1928.

UNITED, STATES PATENT OFFIOE.

EDWARD A. NILL, OF CLEVELAND, OHIO, ASSIGNOB OF ONE-THIRD TO rnnnnnrcxc.

AGREE, OF CLEVELAND HEIGHTS, OHIO, AND ONE-THIRD TO JAMES B. DALL, OI

NOBWALK, OHIO.

LUBRICATING COMPOSITION.

Application filed May 4, 1828. Serial No. 636,639.

I The present invention relates to certain new and useful improvements1n the manufacture of lubricants and similar oil and wax compounds whichare adapted to be 5 used for lubricating and analogous purposes. In acopending applicatlon for Letters Patent of the United States, SerialNo. 585,527, filed August 31, 1922, which has now matured into PatentNo. 1,17,077,

l granted February 8, 1927, I have disclosed a method of producing asolidified oil or grease lubricant without the use of soap, thesolidifying agent, however, being of a saponifiable nature. I have nowmade a 1 further improvement in the lubricating quality of solidifiedoils by the use of neutral anilids of fatty acids, such as the anilidsof palmitic, stearic and arachidic aclds. These anilids, although beingderivatives 'of fatty acids, are entirely neutral bodiesof hydrocarboncharacteristics, and possess ng in themselves a lubricating value.Aniline oil is a well known example of an aromatic base, and stearanilidis a product which can zb be broadly termed an acidyl derivative of anaromaticbase.

Anilids are formed by the union of a fatty acid with aniline oil,accordin to a reaction similar to that given as fol ows which is for thespecific combination of stearic acid and aniline oil.

Stearic acid. Aniline oil. Stearanilid. Water.

GISHSBOZ e s z 24 41 2 .1 have found that it is extremely difficult orpractically impossible to efiect the union of stearic acid with anilineoil to form stearanilid in quantitative yields by merely mixing the twosubstances and heating them, as the aniline oil boils or distills at atemperature much below that to which the acid must be heated for a freechemical union of the substances and under the high temperaturesnecessary to effect this union one molecule of water is given off forevery molecule of stearanilid formed. Furthermore, aniline is of apoisonous nature, so that it is necessary to form the union in a closedvessel, and just merely boiling the stearic 5o acid with thequantitative amount of aniline oil at the boiling point of aniline oilwill not sufiice to bring the two substances into chemical union insuflicient quantities for practical yields. Besides the formation andcondensation of water causes a considerable amount of agitation withinthe vessel so that the process cannot be controlled without the masscontinually boiling over.

The foregoing difiiculties have been over-. come by a s ecial processwhich I have discovered, an while any suitable or a propriate form of aparatus can be employed for carrying on t e process, one possible form ofapparatus is shown by the diagrammatic figure on the accompanyingdrawing.

Referring to the drawing, the numeral 1 designates a wrought ironvertical still in which two hundred and-eighty-four (284 parts ofcommercial stearic acid are place A second still 2 is also utilized, andone hundred and elghty-six (186) parts of commercial aniline oil areplaced in this second still. A vapor pipe 3 leads from the top of domeof the second still 2 to the top of the first still 1, and extendsdownwardly through the still 1 to a point slightly spaced from thebottom thereof. The discharge end of the vapor pipe 3 thus extendsdownwardly below the surface of the stearic acid in the still 1. Each ofthe stills is provided with a thermometer 4, and some means such as aburner 5 is provided for heating each of the stills. The still 2 whichcontains aniline oil is heated to a temperature of from 182 C. to 189C., while the still 1 containing the stearic acid is heated to atemperature of about 235 C., the most favorable working range oftemperature being from 230 C. to 240 C.

The aniline oil in the still 2 is heated to the boiling point, and thevapors pass over into the heated stearic acid in the still 1. Thereaction commences as soon as the aniline vapors begin to pass into themelted acid, providing the latter has been heated to the propertemperature, as indicated above.

A vapor pipe 6 leads from the still 1 to a condenser 7 and a suitablereceptacle 8 is provided to receive the liquid discharged from thecondenser. The water of forma- 100 tion along with any unattachedaniline passes over through the condenser 7 and is collected in thereceptacle 8. The unattached or uncombined aniline oil is thusrecovered, s z that it can be used in a subsequent oper- 105 a ion.

The speed of the reaction is entirely dependent on the rapidity ofdistillation of the aniline oil, and at first practically all of theaniline vapors combine with the stcaric acid, although as the operationcontinues the proportion of aniline oil carried over with the water offormation increases and the quantity of water going over decreases, thedistillation being continued until no more Water goes over, when thereaction is complete and all of the stearic acid has been converted intostearanilid. The aniline oil distillation is then discontinued, and thestearic acid still is heated until no more aniline oil appears at thedischarge end of the condenser 7. This assures the removal of all excessof aniline oil from the product, and the result is a quantitative yieldof stearanihd, which has been found to have a melting point of from C.to 93 0., according to the purity of the products employed. The

stills 1 and 2 each have an inlet 9 and an outlet 10, which arecontrolled in the usual manner by valves or cocks, so that they can beopened and closed as desired. The resulting ield of stearanilid can bedrawn off from the still 1 through the outlet 10.

In the foregoing example I have used stearic acid, although it will beunderstood that other fatty acids, such as, palmitic acid and arachidicacid can be employed. The product will be an anilid of the particularfatty acidthat is used, and in my experiments I have found that thesefatty anilids are nonsaponifiable. These anilids althou h beingderivatives of fatty acids, are entire ly neutral bodies of hydrocarboncharacteristics. Being neutral, the anilids .will not have any corrosiveaction on metal, and can be used in lubricants or other substancescoming into contact with metals without any of the objectionable resultswhich are incident to the fatty acids themselves,"the latter acting veryreadily upon metal surfaces as is well known. The anilids thus have avery decided advantage over fatty substances when used in lubricants,since they do not corrode the metal surfaces.

These anilids have a high melting point which is above 200 F., and onlya small percentage of these anilids is required to solidify oils to theconsistency of grease, and lubricating oils of any desired viscositycanbe reduced to a semi-fluid or solid consistency. For example I find thatby melting 10% of stearanilid with of 28 B. parafiine oil a lightcolored transparent lubricant is obtained, and with 7% of stearanilid.and 93% of cylinder oil a transparent eenish lubricant results. Theformer luricant is suitable for bearings running at high speeds, andunder light loads, while the latter grease is more suitable for use inbearings which run at low speeds under heavy loads, or for use inordinary grease cups or high pressure lubricating systems. It will beunderstood that I do not limit the use of the anilid base to thepercentages given in the foregoing examples, or to combination anilidbase canbe produced in any suitable.

manner, being the product of chemical reaction between aniline oil andone of the fatty acids.

In order to produce a finished lubricant oi smooth and uniform texture,I preferably bring the anilid and the wax or oil together and heat themixture to a temperature of about 205 F. All of the anilid is therebydissolved, after which the mixture is suddenly chilled to a temperaturebelow the solidifying point thereof. This can be accomplished in anysuitable manner, although 1 have found that one convenient way of doingthis is to use a cooling cylinder similar to those which are commonlyemployed in chilling lard compounds.

As another example of the manner in which this invention can be put intopractice, I might mention that a lubricant well adaptable for use inroller and ball bearings can be produced by dissolving a smallpercentage of stearanilid in petrolatum. A mixture of 5% stearanilidwith 95% zero oil, that is a mineral oil having a viscosity of 500seconds Saybolt at F., forms a transparent lubricant of properconsistency for use in ordinary grease cups or a hi h pressure gun. Amixture of 3% stearanihd and 97% zero oil having a viscosity of 2000seconds Saybolt, at 100 F., forms a suitable lubricant for gears andbearings carrying extremely heavy pressures. Even gasoline, kerosene andthe like can be used with the stearanilid. While they have littlelubricating value in themselves, they may be employed as vehicles tocarry the stearanilid and oil mixture to parts which are difficult toreach. For example, a mixture of 25 parts stearanilid'and 75 parts ofkerosene forms a paste suitable for use in the lubrication ofphonographs.

The products of the invention are not restricted to lubricants, since Ihave found that by mixing stearanilid with parafline wax or a mixture ofstearic acid and paraffine wax, a product suitable for molding intocandles is produced. The particular ad- IOU vantage of this candlemaking product is that the stearanilid gives it a comparativel highmelting point, so that the candles wi 1 be harder and better adapted toresist the softening influences of a warm atmosphere. Candlesmanufactured from this compound will maintain their shape under allusual atmospheric and climatic conditions, and will not soften and bendover under the influence of a warm atmosphere. While stearanilid costsslightly more than stearic acid, it serves as a cheaper substitute forthe latter in this candle making compound, since a smaller amount isneeded to produce parafline candles of proper hardness or stiffness.

For illustrative purposes in describing the invention, I have shown anumber of specific ways in which the invention can be used to producecommercial products, although I wish it to be understood that I do notrestrict myself to the details of the process or to the particularproducts mentioned, since many other useful products can be obtained byvarious combinations and mixtures of an anilid with different kinds ofoils and waxes, the anilid serving to stiffen the consistency of the oilor raise the melting point of the wax.

A method of producing the lubricating composition of the presentinvention is disclosed and claimed in my copending application, SerialNo. 238,267, filed December 7 1927, which is a continuation in part ofthis application.

Having thus described my invention what WVhiCh is substantially freefrom water and consists of paraffine oil having a neutral stearanilidmixed therewith to stifien the consistency thereof.

2. A lubricant which is free from water and comprises cylinder oil andneutral stearanilid mixed with the cylinder oil to stiffen theconsistency thereof.

3. A lubricant which is free from water and comprises approximatelyninety-three percent (93%) cylinder oil and approximately seven percent(7%) neutral stearanilid, the stearanilid serving to stiffen theconsistency of the cylinder oil.

. 4. A lubricating composition which is substantially free from waterand comprises a mineral oil having dissolved therein a neutral anilid ofa fatty acid to stiffen the consistency and raise the melting point ofthe composition.

5. A lubricating composition which is substantially free from water andcomprises a mineral oil having stearanilid dissolved therein to stiffenthe consistency thereof.

6. A lubricatin composition which is substantially free from water andcomprises cylinder oil having a neutral anilid of a fatty acid dissolvedtherein to stiffen the consistency and raise the melting point of thecomposition.

In testimony whereof I afiix my signature.

EDWARD A. NILL.

